Reaktion #83163

ord-002083350cc34e8dbe3e7428d2f0b9f3

Reaktionsgleichung

CCO[Si](CCCN)(OCC)OCC
3-aminopropyltriethoxysilane
CCN(CC)CC
triethylamine
C=CC(=O)Cl
acryloyl chloride
C=C(CCC[Si](OCC)(OCC)OCC)C(N)=O
liquid
Ausbeute 77.0%
C=C(CCC[Si](OCC)(OCC)OCC)C(N)=O
3-(Triethoxysilyl)propylacrylamide
Ausbeute 77.0%

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added dropwise
  2. 2
    workup.ADDITIONAfter completion of addition the reaction mixture
  3. 3
    Filtrationfiltered
  4. 4
    EinengenThe filtrate was concentrated to an oil
  5. 5
    workup.ADDITIONdiluted with hexane (100 mL)
  6. 6
    Filtrationfiltered
  7. 7
    EinengenThe resulting filtrate was concentrated to oil
  8. 8
    workup.DISTILLATIONdistilled in vacuo

Vorschrift

To a solution of acryloyl chloride (8.5 mL, 105 mmol) in dry dichloromethane (250 mL) cooled to 0° C. was added dropwise a mixture of 3-aminopropyltriethoxysilane (23.5 mL, 100 mmol) and triethylamine (13.9 mL, 100 mmol) in dichloromethane (50 mL). After completion of addition the reaction mixture was stirred for 30 min, then filtered. The filtrate was concentrated to an oil, diluted with hexane (100 mL) and filtered. The resulting filtrate was concentrated to oil and distilled in vacuo. The product was obtained as a viscous liquid (21.2 g, 77%), b.p. 142-145/1 mm Hg.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05624711uspto-grants-1997_04